CN114985756B - Method for preparing silver nanowire based on small molecular phenolic acid at room temperature - Google Patents
Method for preparing silver nanowire based on small molecular phenolic acid at room temperature Download PDFInfo
- Publication number
- CN114985756B CN114985756B CN202210553501.7A CN202210553501A CN114985756B CN 114985756 B CN114985756 B CN 114985756B CN 202210553501 A CN202210553501 A CN 202210553501A CN 114985756 B CN114985756 B CN 114985756B
- Authority
- CN
- China
- Prior art keywords
- silver
- solution
- cotton fabric
- room temperature
- small molecular
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a method for preparing silver nanowires based on small molecular phenolic acid at room temperature, which comprises the steps of taking small molecular phenolic acid as a reducing agent, taking polyvinylpyrrolidone as a template agent, and reducing a silver source under the room temperature condition to prepare silver nanowires; and depositing the silver nanowires on the surface of the cotton fabric by a dipping-rolling-drying method to prepare the conductive cotton fabric, wherein the square resistance of the conductive cotton fabric is 0.23-0.54 ohm/sq. The method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature has simple process flow, can be performed at room temperature, and avoids high-temperature and high-pressure conditions, is environment-friendly, saves energy and reduces energy consumption compared with the prior main silver nanowire preparation methods such as a polyol method, a solvothermal method and the like; and the required equipment is simple, the material size is unlimited, the equipment cost is low, and the large-scale production can be realized.
Description
Technical Field
The invention belongs to the technical field of silver nanowires, and relates to a method for preparing silver nanowires at room temperature based on small molecular phenolic acid.
Background
Currently, the preparation methods of silver nanowires mainly include Ultraviolet (UV) light irradiation, template, solvothermal, polyol, and the like. The ultraviolet irradiation method is a photo-reduction method, which is a photo-reduction method of inducing silver source reduction under the condition of ultraviolet irradiation by adding a proper surfactant as a protective agent. However, only the reactant contacting with ultraviolet light can be triggered and reduced to the final product, and the problems of uneven product, low reduction efficiency and the like are easy to occur. The template method adjusts the shape of the final product by controlling the shape of the template, and is classified into a hard template method and a soft template method. The hard template method has strong controllability, but needs a prefabricated template, the purification process is complex, the purification process of the soft template method is convenient, but the form of the product is difficult to control. The polyol method and the solvothermal method have simple processes and high yield, can realize large-scale production, and are the main two methods for industrially producing the silver nanowires at present. However, these two methods often require conditions such as high temperature and high pressure, and a large amount of chemical agents such as ethylene glycol, propylene glycol or glycerol, which are liable to pollute the environment, are often introduced as reducing agents and solvents. In recent years, along with the increasingly prominent environmental problems, the green development concept is in deep focus, and the environment-friendly high-benefit preparation process with energy conservation and emission reduction becomes a research hotspot of modern scholars.
CN113385686a discloses a method for preparing silver nanowires with high length-diameter ratio with the aid of organic amine hydrochloride. Adding silver nitrate-glycol solution into the mixed solution, heating to 110-180 ℃ and reacting for 2-12 h, cooling to room temperature, and collecting precipitate to obtain silver nanowires with high length-diameter ratio; the mixed solution is obtained by uniformly mixing a polyvinylpyrrolidone-ethylene glycol solution and an organic amine hydrochloride-ethylene glycol solution; the diameter size of the prepared silver nanowire is mainly 100-150 nm, the length is more than 80 mu m, however, the whole synthesis process needs higher temperature and time, and the energy consumption is high.
CN111922359a discloses a method for preparing pure silver nanowires. Firstly preparing a solution A (polydiene dimethyl ammonium chloride glycol solution) and a solution B (silver nitrate glycol solution), then dropwise adding an equal volume of solution B into the solution A under magnetic stirring, magnetically stirring the mixed solution at room temperature for 10-20 min, heating to 160-200 ℃ and reacting for 6-10 hours to obtain a product; cooling the product at room temperature, separating by a centrifuge, washing the centrifuged product, and dispersing the washed product in ethanol; the prepared silver nanowire has quite pure surface and good conductivity and light transmittance. However, the long-time high-temperature reaction causes the production to consume more energy, has great potential safety hazard and difficult control of the reaction process, and the obtained silver nanowires have larger size difference and have certain environmental pollution due to the use of more harmful organic solvents.
CN113210623a discloses a method for preparing pure silver nanowire with controllable length-diameter ratio by microwave-assisted synthesis, which comprises the following steps: heating glycol, uniformly mixing with glycol solution of halide and glycol solution of nitrate, and preserving heat; mixing with glycol solution of silver nitrate, placing into a microwave digestion instrument, heating at 110-150 ℃ with microwave frequency of 300-900 w and microwave time of 30-60 min, washing and centrifuging the obtained solution, and dispersing in solvent again to obtain pure silver nanowires. The higher microwave temperature brings more energy consumption and has low economic benefit.
Therefore, the development of a method for synthesizing the silver nanowire with high length-diameter ratio under mild conditions without high pressure and high temperature is one of the directions of urgent breakthrough of researchers, and the synthesis process is simple, energy-saving and environment-friendly.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing silver nanowires based on small molecular phenolic acid at room temperature.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature is to prepare the silver nanowire by reducing a silver source at room temperature (25-30 ℃) by taking the small molecular phenolic acid as a reducing agent and polyvinylpyrrolidone (PVP) as a template agent.
As a preferable technical scheme:
the method for preparing the silver nanowire at room temperature based on the small molecular phenolic acid is characterized in that the small molecular phenolic acid is caffeic acid, ferulic acid or chlorogenic acid.
The method for preparing silver nanowires based on small molecular phenolic acid at room temperature as described above, the molecular weight of polyvinylpyrrolidone is 20000 ～ 1300000 daltons.
The method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature has the silver source of silver nitrate, silver bromide or silver sulfate.
The method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature has the advantages that the diameter of the silver nanowire is 40-60 nm, and the length of the silver nanowire is 40-60 mu m; the silver nanowires are deposited on the surface of the cotton fabric through a dipping-rolling-drying method to prepare the conductive cotton fabric, and the square resistance of the conductive cotton fabric is 0.23-0.54 ohm/sq.
The specific steps of the silver nanowire used for conducting finishing of cotton fabric are as follows:
(1) Scouring and cleaning cotton fabric to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing the cotton fabric after washing;
(2) Immersing the cotton fabric in the step (1) in water for ultrasonic treatment at room temperature for 10-20 min, wherein the surface of the fiber is roughened by the ultrasonic acoustic cavitation, and meanwhile, the residual air in the fabric interweaving structure is discharged, so that the adsorption effect of the surface of the cotton fabric is greatly enhanced, and the contact and combination between the cotton fabric and silver nanowires are facilitated;
(3) Preparing the synthesized silver nanowire into a silver nanowire aqueous solution with the mass concentration of 6-12 g/L, and dispersing the silver nanowire aqueous solution for 3-5 min by ultrasonic waves; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature of 80 ℃ in an oscillating water bath kettle for 20-30 min, taking out the rolled solution, drying in a 60 ℃ oven, and repeating the soaking-rolling-drying process for 2-3 times; finally, immersing the obtained fabric in a chloride aqueous solution for 30-60 s, washing the fabric with deionized water for 10-20 s, repeating the washing for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric (the prepared conductive cotton fabric is further soaked in a chloride ion solution, and chloride ions and dissolved oxygen molecules existing in the solution dissolve silver ions from the surface of silver nanowires and are dissociated through the solution to redeposit at nodes, so that node resistance and cotton fabric surface sheet resistance are reduced).
The temperature of the ultrasonic dispersion in the step (3) is room temperature, and the ultrasonic frequency is 40-60KHz; the rolling surplus rate of the rolling solution is 100-150%; the chloride is sodium chloride, potassium chloride or lithium chloride, and the mass fraction of the aqueous solution is 10-20%.
The method for preparing the silver nanowire at room temperature based on the small molecular phenolic acid comprises the following specific preparation steps:
(1) Respectively preparing silver source solution with the concentration of 0.5-3 mol/L, micromolecular phenolic acid aqueous solution with the concentration of 2-3 g/L and polyvinylpyrrolidone solution with the concentration of 0.01-0.05 g/L;
(2) Adding a silver source solution into a polyvinylpyrrolidone solution, and uniformly stirring and mixing to obtain a mixed solution;
(3) Adding small molecular phenolic acid aqueous solution into the mixed solution obtained in the step (2), stirring at room temperature for reaction for 5-10 min, heating to 28-30 ℃, and standing for reaction for 3-4 h;
(4) And (3) centrifugally separating the solution after the reaction in the step (3), taking the sediment at the lower layer, cleaning, and repeating the steps of centrifugation and cleaning for 2-4 times to obtain the silver nanowires.
According to the method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature, the volume ratio of the silver source solution to the polyvinylpyrrolidone solution in the step (2) is 1:40-80;
the volume ratio of the small molecular phenolic acid aqueous solution to the mixed solution in the step (3) is 7:41-81.
According to the method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature, the stirring speed in the step (2) is 500-600 r/min, and the step of rapid stirring is used for enabling the silver source solution to be rapidly and uniformly dispersed, and the mixing time is 15-20 min;
the stirring speed in the step (3) is 100-300 r/min, and the purpose of the slow stirring in the step is to prevent the rapid contact of the reducing agent and the silver source due to the too fast stirring, the too fast reaction, the reduction of a large amount of silver ions into silver atoms for a long time and the rapid agglomeration into large silver crystal nuclei, so that silver particles or short and coarse silver nano rods are accompanied in addition to nanowires in the finally synthesized solution. The slow stirring is beneficial to the acquisition of silver nanowires, and the result is verified by a controlled variable method in experiments.
According to the method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature, the small molecular phenolic acid aqueous solution is added in the step (3) in a dropwise adding mode, and the dropwise adding speed is 2.8-20 mL/min.
The method for preparing silver nanowires based on small molecular phenolic acid at room temperature as described above, wherein the cleaning in the step (4) means: ethanol is used for cleaning, and deionized water is used for cleaning.
The principle of the invention is as follows:
the carboxyl group in the biomass small molecular phenolic acid can easily capture positively charged Ag ions from the solution and form relatively stable complexes with the positively charged Ag ions. However, since phenolic hydroxyl groups in phenolic acids have reducing property, silver ions trapped in the complex are reduced to silver atoms and released. Silver atoms begin to nucleate slowly and unevenly. As the reaction proceeds, the reduced silver atoms grow more and aggregate into primary silver crystals. Subsequently, oxygen in c=o in the polyvinylpyrrolidone structure forms a silver-oxygen bond with Ag (silver crystal), and since the surface free energy of the Ag (111) crystal plane is smaller than that of the Ag (100) crystal plane, polyvinylpyrrolidone is coated on the Ag (100) crystal plane, that is, the Ag (100) plane forms a silver-oxygen bond with polyvinylpyrrolidone, and is covered. Since polyvinylpyrrolidone belongs to a polymer chain, the surface of a silver simple substance (100) which is continuously and newly generated is combined with oxygen in C=O on polyvinylpyrrolidone, and the surface of Ag (111) is connected with other surfaces of Ag (111), so that the generated silver twin crystal grows linearly in one dimension along the surface of (111), and silver nanowires are gradually generated.
The method of the present invention can prepare silver nanowires at room temperature because: firstly, alcohols such as ethylene glycol are mainly used as reducing agents in the prior art, and compared with the alcohols, the small molecular phenolic acid in the invention has stronger reducibility. Because of the existence of benzene ring and double bond on the side chain of benzene ring in the phenolic acid compound structure, a large conjugated system is often formed in the molecule, and because of the existence of carboxyl, the electron withdrawing capability of the conjugated system is larger. In the phenolic hydroxyl C-O-H structure, an oxygen atom contains a lone pair p electron, the p electron cloud is overlapped with a large pi electron cloud in a conjugated system from the side surface, the p electron cloud on the oxygen atom is transferred to a benzene ring due to the electron-withdrawing effect of the conjugated system, and the electron cloud among hydrogen atoms is transferred to the direction of the oxygen atom, so that an O-H bond on the phenolic hydroxyl is easy to break and easy to oxidize, and a O-benzoquinone structure is generated. The alcohol hydroxyl is generally connected with alkane or alkene, at most, p-pi conjugation can be realized only in a small range, and the O-H bond energy is large and is difficult to oxidize. The dissociation energy (BED) of the O-H bond in the phenolic hydroxyl group of the phenolic acid compound is much smaller than that of the alcoholic hydroxyl group of the glycol (the BED of the O-H bond in the phenolic hydroxyl group of the phenolic acid compound is generally about 200kJ/mol to 400 kJ/mol). Therefore, phenolic acid compounds are more reducing than alcohols, and metal ions are more easily reduced into simple substances, so that the higher reaction temperature is not required like alcohols. Secondly, carboxyl anions in the small molecular phenolic acid capture positively charged Ag from the solution through electrostatic complexation + The electrons freely displaced between the conjugated ring and the side chain double bond gradually get closer to Ag under the influence of electrostatic force + ，Ag + The electrons are easy to obtain,is reduced to silver atoms, which to some extent can promote the rapid and orderly reduction of silver ions without the need for higher environmental energies. In conclusion, the silver nanowire can be prepared at room temperature under the reaction condition without high temperature.
The beneficial effects are that:
(1) The method for preparing the silver nanowire based on the small molecular phenolic acid at room temperature has simple process flow, can be performed at room temperature, and avoids high-temperature and high-pressure conditions, is environment-friendly, saves energy and reduces energy consumption compared with the prior main silver nanowire preparation methods such as a polyol method, a solvothermal method and the like;
(2) The preparation method used in the invention has the advantages of simple equipment, no limitation on the size of the material, low equipment cost and large-scale production;
(3) According to the invention, polyvinylpyrrolidone is added into the reaction mixed solution as a surfactant and a protective agent, and the coating effect of PVP can prevent the aggregation of silver particles in the process of reducing silver ions into nano silver particles. Meanwhile, PVP also serves as a blocking agent and a soft template to promote the growth of silver twin crystal orientation one-dimensional structure.
Drawings
FIG. 1 is an SEM image of silver nanowires obtained in example 1;
FIG. 2 is a TEM image of silver nanowires obtained in example 2;
FIG. 3 is an XRD pattern for silver nanowires produced in example 3;
fig. 4 shows the results of the conductivity and laundering resistance tests of AgNW/cotton fabrics in examples 8 to 11, as measured by the ST-2258C type multifunctional digital four-probe tester.
Detailed Description
The invention is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Further, it is understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the contents of the present invention, and such equivalents are also within the scope of the claims appended hereto.
Room temperature in the examples below refers to 25 ℃.
Example 1
A method for preparing silver nanowires based on small molecular phenolic acid (caffeic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver nitrate solution with the concentration of 1mol/L, a caffeic acid aqueous solution with the concentration of 2.4g/L and a polyvinylpyrrolidone solution with the concentration of 0.04 g/L;
wherein the molecular weight of polyvinylpyrrolidone is 40000 daltons;
(2) Adding silver nitrate solution into polyvinylpyrrolidone solution, stirring at 600r/min for 20min, and mixing to obtain mixed solution;
wherein, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution is 1:60;
(3) Dropwise adding an aqueous solution of caffeic acid into the mixed solution obtained in the step (2) at a speed of 2.8mL/min, stirring at a speed of 280r/min at room temperature for reaction for 5min, and then heating to 28 ℃ for standing reaction for 4h;
wherein the volume ratio of the aqueous solution of the caffeic acid to the mixed solution is 7:61;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 2 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 46+/-2 nm, the length is 49+/-3 mu m, and a scanning electron microscope chart is shown in figure 1.
Example 2
A method for preparing silver nanowires based on small molecular phenolic acid (caffeic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver nitrate solution with the concentration of 1mol/L, a caffeic acid aqueous solution with the concentration of 2.4g/L and a polyvinylpyrrolidone solution with the concentration of 0.03 g/L;
wherein the polyvinylpyrrolidone has a molecular weight of 58000 daltons;
(2) Adding silver nitrate solution into polyvinylpyrrolidone solution, stirring at 600r/min for 20min, and mixing to obtain mixed solution;
wherein, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution is 1:60;
(3) Dropwise adding an aqueous solution of caffeic acid into the mixed solution obtained in the step (2) at a speed of 2.8mL/min, stirring at a speed of 280r/min at room temperature for reaction for 5min, and then heating to 28 ℃ for standing reaction for 3.5h;
wherein the volume ratio of the aqueous solution of the caffeic acid to the mixed solution is 7:61;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 3 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 50+/-3 nm, the length is 52+/-2 mu m, and the transmission electron microscope chart is shown in figure 2.
Example 3
A method for preparing silver nanowires based on small molecular phenolic acid (caffeic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver nitrate solution with the concentration of 1mol/L, a caffeic acid aqueous solution with the concentration of 2.4g/L and a polyvinylpyrrolidone solution with the concentration of 0.02 g/L;
wherein the molecular weight of polyvinylpyrrolidone is 40000 daltons;
(2) Adding silver nitrate solution into polyvinylpyrrolidone solution, stirring at 600r/min for 20min, and mixing to obtain mixed solution;
wherein, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution is 1:60;
(3) Dropwise adding an aqueous solution of caffeic acid into the mixed solution obtained in the step (2) at a speed of 2.8mL/min, stirring at a speed of 280r/min at room temperature for reaction for 5min, and then heating to 28 ℃ for standing reaction for 3.5h;
wherein the volume ratio of the aqueous solution of the caffeic acid to the mixed solution is 7:61;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 4 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 54+/-5 nm, the length is 46+/-4 mu m, and the X-ray diffraction diagram is shown in figure 3.
As can be seen from FIG. 3, the X-ray diffraction peaks are quite clear, the peak types all show the characteristics of narrow peaks and higher intensity, which indicates that the crystallinity of the prepared silver nanowire is better; 4 obvious diffraction peaks appear in the XRD diagram, each peak corresponds to 04-0783 numbered in the JCPDS standard card, each peak corresponds to the crystal face diffraction peaks of the face-centered cubic elemental silver (111), (200), (220), (311) and (222), and no other impurity peaks exist in the diagram; in addition, the ratio of the (111) plane peak to the (200) plane peak relative diffraction peak intensity can be calculated from the data of fig. 3 to be 4.95, which is greater than the theoretical (111) plane and (200) plane relative diffraction peak intensity of 2.50, and meanwhile, the (111) plane diffraction peak intensity is also far greater than the (220) plane and the (311) plane, which indicates that the growth rate of the (111) plane of the crystal is greater than the growth rate of other planes in the reaction process, and the silver nanowire is obtained by one-dimensional growth.
Example 4
A method for preparing silver nanowires based on small molecular phenolic acid (caffeic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver nitrate solution with the concentration of 1mol/L, a caffeic acid aqueous solution with the concentration of 2.4g/L and a polyvinylpyrrolidone solution with the concentration of 0.01 g/L;
wherein the molecular weight of polyvinylpyrrolidone is 1300000 daltons;
(2) Adding silver nitrate solution into polyvinylpyrrolidone solution, stirring at 600r/min for 20min, and mixing to obtain mixed solution;
wherein, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution is 1:60;
(3) Dropwise adding an aqueous solution of caffeic acid into the mixed solution obtained in the step (2) at a speed of 2.8mL/min, stirring at a speed of 280r/min at room temperature for reaction for 5min, and then heating to 28 ℃ for standing reaction for 4h;
wherein the volume ratio of the aqueous solution of the caffeic acid to the mixed solution is 7:61;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 4 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 56+/-2 nm, and the length is 59+/-3 mu m.
Example 5
A method for preparing silver nanowires based on small molecular phenolic acid (ferulic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing silver bromide solution with the concentration of 0.5mol/L, ferulic acid aqueous solution with the concentration of 2g/L and polyvinylpyrrolidone solution with the concentration of 0.05 g/L;
wherein the molecular weight of polyvinylpyrrolidone is 40000 daltons;
(2) Adding silver bromide solution into polyvinylpyrrolidone solution, stirring at 500r/min for 15min, and mixing uniformly to obtain mixed solution;
wherein, the volume ratio of the silver bromide solution to the polyvinylpyrrolidone solution is 1:40;
(3) Dropwise adding an aqueous solution of ferulic acid into the mixed solution obtained in the step (2) at a speed of 10mL/min, stirring at room temperature at a speed of 100r/min for reaction for 10min, and then heating to 30 ℃ for standing reaction for 3.5h;
wherein the volume ratio of the ferulic acid aqueous solution to the mixed solution is 7:41;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 3 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 44+/-3 nm, and the length is 51+/-2 mu m.
Example 6
A method for preparing silver nanowires based on small molecular phenolic acid (chlorogenic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver sulfate solution with the concentration of 2mol/L, a chlorogenic acid aqueous solution with the concentration of 3g/L and a polyvinylpyrrolidone solution with the concentration of 0.02 g/L;
wherein the molecular weight of polyvinylpyrrolidone is 40000 daltons;
(2) Adding the silver sulfate solution into the polyvinylpyrrolidone solution, stirring at the speed of 500r/min for 15min, and uniformly mixing to obtain a mixed solution;
wherein, the volume ratio of the silver sulfate solution to the polyvinylpyrrolidone solution is 1:80;
(3) Dropwise adding chlorogenic acid aqueous solution into the mixed solution obtained in the step (2) at a speed of 20mL/min, stirring at room temperature at a speed of 200r/min for reaction for 10min, and then heating to 28 ℃ for standing reaction for 3h;
wherein the volume ratio of chlorogenic acid aqueous solution to the mixed solution is 7:81;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 4 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 53+/-4 nm, and the length is 47+/-4 mu m.
Example 7
A method for preparing silver nanowires based on small molecular phenolic acid (ferulic acid) at room temperature comprises the following specific preparation steps:
(1) Respectively preparing a silver nitrate solution with the concentration of 3mol/L, a ferulic acid aqueous solution with the concentration of 2.4g/L and a polyvinylpyrrolidone solution with the concentration of 0.03 g/L;
wherein the polyvinylpyrrolidone has a molecular weight of 58000 daltons;
(2) Adding silver nitrate solution into polyvinylpyrrolidone solution, stirring at 600r/min for 20min, and mixing to obtain mixed solution;
wherein, the volume ratio of the silver nitrate solution to the polyvinylpyrrolidone solution is 1:60;
(3) Dropwise adding an aqueous solution of ferulic acid into the mixed solution obtained in the step (2) at a speed of 15mL/min, stirring at a speed of 300r/min at room temperature for reaction for 5min, and then heating to 30 ℃ for standing reaction for 3h;
wherein the volume ratio of the ferulic acid aqueous solution to the mixed solution is 7:61;
(4) Centrifugally separating the solution reacted in the step (3) at a centrifugal speed of 5000rmp, taking a lower layer precipitate, cleaning the lower layer precipitate with ethanol, cleaning the lower layer precipitate with deionized water, and repeating the steps of centrifugation and cleaning for 4 times to obtain silver nanowires;
the diameter of the prepared silver nanowire is 51+/-2 nm, and the length is 51+/-3 mu m.
Example 8
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 10min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 1 is prepared into an aqueous silver nanowire solution with the mass concentration of 6g/L, and is dispersed for 3min at room temperature under the ultrasonic wave of 40KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 30min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 3 times; finally, immersing the obtained fabric in sodium chloride aqueous solution for 45s, washing with deionized water for 20s, repeating for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 150%; the mass fraction of the sodium chloride aqueous solution is 10%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.54+/-0.06 ohm/sq.
Example 9
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 10min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 2 is prepared into an aqueous silver nanowire solution with the mass concentration of 8g/L, and is dispersed for 3min at room temperature under the ultrasonic wave of 50KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 30min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 3 times; finally, immersing the obtained fabric in a potassium chloride aqueous solution for 45s, washing the fabric with deionized water for 20s, repeating the washing process for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 150%; the mass fraction of the potassium chloride aqueous solution is 10%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.33+/-0.09 omega/sq.
Example 10
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 20min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 3 is prepared into an aqueous silver nanowire solution with the mass concentration of 10g/L, and is dispersed for 5min at the room temperature under the ultrasonic wave of 60KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 30min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 2 times; finally, immersing the obtained fabric in lithium chloride aqueous solution for 45s, washing with deionized water for 20s, repeating for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 150%; the mass fraction of the lithium chloride aqueous solution is 10%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.26+/-0.04 ohm/sq.
Example 11
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 20min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 4 is prepared into a silver nanowire aqueous solution with the mass concentration of 12g/L, and is dispersed for 5min at the room temperature under the ultrasonic wave of 60KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 30min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 2 times; finally, immersing the obtained fabric in sodium chloride aqueous solution for 60s, washing with deionized water for 20s, repeating for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 150%; the mass fraction of the sodium chloride aqueous solution is 10%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.23+/-0.02 ohm/sq.
Respectively placing the conductive cotton fabrics prepared in the examples 8-11 into 2g/L soap solution, respectively placing 10 steel balls, respectively washing for 2 times, 4 times, 8 times and 10 times in a Wash Tec-P type washing fastness tester at 45 ℃ with 15min as a washing period, and testing the resistance of each conductive cotton fabric by adopting an ST-2258C type multifunctional digital four-probe tester, wherein the test results are shown in figure 4; as can be seen from fig. 4, the conductive cotton fabric prepared by the method of the present invention has good washing stability.
Example 12
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 10min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 5 is prepared into an aqueous silver nanowire solution with the mass concentration of 8g/L, and is dispersed for 4min at room temperature under the ultrasonic wave of 50KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 20min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 3 times; finally, immersing the obtained fabric in a potassium chloride aqueous solution for 60s, washing the fabric with deionized water for 10s, repeating the washing process for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled is 100 percent; the mass fraction of the potassium chloride aqueous solution is 20%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is 0.80+/-0.04 ohm/sq.
Example 13
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 20min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 6 is prepared into an aqueous silver nanowire solution with the mass concentration of 10g/L, and is dispersed for 4min at room temperature under the ultrasonic wave of 40KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 25min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 2 times; finally, immersing the obtained fabric in lithium chloride aqueous solution for 45s, washing for 15s by deionized water, repeating for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 120%; the mass fraction of the lithium chloride aqueous solution is 10%;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.58+/-0.02 ohm/sq.
Example 14
A method for conducting finishing of cotton fabrics by silver nanowires comprises the following specific steps:
(1) Cleaning cotton fabrics:
preparing 2g/L soap solution, boiling cotton fabric at 100 ℃ for 30min at a bath ratio of 1:60, washing with deionized water for 3 times to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing after washing;
(2) Pretreatment of cotton fabric:
cutting the cotton fabric in the step (1) into 4 multiplied by 4cm blocks, and immersing the blocks in water for ultrasonic treatment at room temperature for 20min;
(3) Conducting finishing:
the silver nanowire synthesized in the example 7 is prepared into a silver nanowire aqueous solution with the mass concentration of 12g/L, and is dispersed for 5min at the room temperature under the ultrasonic wave of 60KHz frequency; soaking the cotton fabric treated in the step (2) into silver nanowire solution, maintaining the temperature in an oscillating water bath kettle for 25min, taking out the rolled solution, drying in a baking oven at 60 ℃, and repeating the soaking-rolling-drying process for 2 times; finally, immersing the obtained fabric in sodium chloride aqueous solution for 30s, washing with deionized water for 20s, repeating for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
wherein the rolling surplus rate when the solution is rolled out is 120%; 15% of sodium chloride aqueous solution by mass;
and (3) testing the square resistance of the prepared conductive cotton fabric by adopting a ST-2258C type multifunctional digital four-probe tester, wherein the square resistance of the conductive cotton fabric is measured to be 0.33+/-0.02 ohm/sq.
Claims (7)
1. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid in the conductive finishing of cotton fabric is characterized in that: taking small molecular phenolic acid as a reducing agent, taking polyvinylpyrrolidone as a template agent, and reducing a silver source under the room temperature condition to prepare silver nanowires; depositing the silver nanowires on the surface of the cotton fabric by a dipping-rolling-drying method to prepare the conductive cotton fabric, wherein the square resistance of the conductive cotton fabric is 0.23-0.54 ohm/sq;
the small molecular phenolic acid is caffeic acid, ferulic acid or chlorogenic acid;
the preparation method of the silver nanowire based on the small molecular phenolic acid at room temperature comprises the following steps:
(1) Respectively preparing a silver source solution with the concentration of 0.5-3 mol/L, a small molecular phenolic acid aqueous solution with the concentration of 2-3 g/L and a polyvinylpyrrolidone solution with the concentration of 0.01-0.05 g/L;
(2) Adding a silver source solution into a polyvinylpyrrolidone solution, and uniformly stirring and mixing to obtain a mixed solution;
(3) Adding a small molecular phenolic acid aqueous solution into the mixed solution obtained in the step (2), stirring at room temperature for reaction for 5-10 min, heating to 28-30 ℃, and standing for reaction for 3-4 h;
(4) Centrifuging the solution reacted in the step (3), taking the lower layer precipitate for cleaning, and repeating the centrifuging and cleaning steps for 2-4 times to obtain silver nanowires;
the step of depositing the silver nanowires on the surface of the cotton fabric by a dipping-rolling-drying method to prepare the conductive cotton fabric is as follows:
(i) Scouring and cleaning cotton fabric to remove natural and artificial impurities on the surface of the cotton fabric, and naturally airing the cotton fabric after washing;
(ii) Immersing the cotton fabric in the step (i) in water, and performing ultrasonic treatment at room temperature for 10-20 min, wherein the surface of the fiber is roughened by the ultrasonic acoustic cavitation, and meanwhile, the residual air in the fabric interweaving structure is discharged, so that the adsorption effect of the surface of the cotton fabric is enhanced, and the contact and combination between the cotton fabric and silver nanowires are facilitated;
(iii) Preparing silver nanowires into silver nanowire aqueous solution with the mass concentration of 6-12 g/L, and performing ultrasonic dispersion for 3-5 min; immersing the cotton fabric treated in the step (ii) into silver nanowire solution, maintaining the temperature of 80 ℃ in an oscillating water bath for 20-30 min, taking out the rolled solution, drying in a 60 ℃ oven, and repeating the soaking-rolling-drying process for 2-3 times; finally, immersing the obtained fabric in a chloride aqueous solution for 30-60 s, washing the fabric with deionized water for 10-20 s, repeating the washing process for 2 times, and drying at 60 ℃ to obtain the conductive cotton fabric;
the temperature of the ultrasonic dispersion in the step (iii) is room temperature, and the ultrasonic frequency is 40-60KHz; the rolling surplus rate when the solution is rolled is 100-150%; the chloride is sodium chloride, potassium chloride or lithium chloride, and the mass fraction of the aqueous solution is 10-20%.
2. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid to the conductive finishing of cotton fabric according to claim 1, wherein the molecular weight of polyvinylpyrrolidone is 20000-1300000 daltons.
3. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid to the conductive finishing of cotton fabric according to claim 1, wherein the silver source is silver nitrate, silver bromide or silver sulfate.
4. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid to the conductive finishing of cotton fabric, which is disclosed in claim 1, is characterized in that the volume ratio of the silver source solution to the polyvinylpyrrolidone solution in the step (2) is 1:40-80;
and (3) the volume ratio of the small molecular phenolic acid aqueous solution to the mixed solution is 7:41-81.
5. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid to the conductive finishing of cotton fabrics, which is disclosed in claim 1, is characterized in that the stirring speed in the step (2) is 500-600 r/min, and the mixing time is 15-20 min;
the stirring speed in the step (3) is 100-300 r/min.
6. The application of the silver nanowire prepared at room temperature based on the small molecular phenolic acid to the conductive finishing of cotton fabrics, which is disclosed in claim 1, is characterized in that the small molecular phenolic acid aqueous solution is added in the step (3) in a dropwise adding mode, and the dropwise adding speed is 2.8-20 mL/min.
7. The use of silver nanowires prepared at room temperature based on small molecular phenolic acids according to claim 1 for conducting finishing of cotton fabrics, wherein the washing in step (4) means: ethanol is used for cleaning, and deionized water is used for cleaning.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210553501.7A CN114985756B (en) | 2022-05-20 | 2022-05-20 | Method for preparing silver nanowire based on small molecular phenolic acid at room temperature |
| PCT/CN2022/109870 WO2023221299A1 (en) | 2022-05-20 | 2022-08-03 | Method for preparing silver nanowires at room temperature on the basis of micromolecular phenolic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210553501.7A CN114985756B (en) | 2022-05-20 | 2022-05-20 | Method for preparing silver nanowire based on small molecular phenolic acid at room temperature |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114985756A CN114985756A (en) | 2022-09-02 |
| CN114985756B true CN114985756B (en) | 2023-07-28 |
Family
ID=83027113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210553501.7A Active CN114985756B (en) | 2022-05-20 | 2022-05-20 | Method for preparing silver nanowire based on small molecular phenolic acid at room temperature |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN114985756B (en) |
| WO (1) | WO2023221299A1 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106392098A (en) * | 2016-10-10 | 2017-02-15 | 苏州经贸职业技术学院 | Preparation method of nanometer silver hydrosol and treatment method for dye wastewater |
| CN114214833A (en) * | 2021-12-09 | 2022-03-22 | 西安理工大学 | Preparation method of flexible conductive fabric sensor based on silver nanowires/graphene |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1236131C (en) * | 2004-02-13 | 2006-01-11 | 黄德欢 | Preparation method of antibiotic textile carrying nano silver |
| CA2728987C (en) * | 2008-05-16 | 2018-12-04 | Verutek Technologies, Inc. | Green synthesis of nanometals using plant extracts and use thereof |
| CN103302306A (en) * | 2013-06-19 | 2013-09-18 | 东南大学 | Method for reducing and preparing functionalized nano-silver based on polyphenol |
| US20150266096A1 (en) * | 2014-03-18 | 2015-09-24 | Blue Nano Inc. | Silver nanowires with thin diameter and high aspect ratio and hydrothermal synthesis method for making the same |
| CN105088755A (en) * | 2015-08-22 | 2015-11-25 | 赵兵 | Preparation method and application of silver nano-particles |
| JP2019212524A (en) * | 2018-06-06 | 2019-12-12 | 三菱製紙株式会社 | Method of treating conductive material |
| CN109954887A (en) * | 2019-03-22 | 2019-07-02 | 扬州大学 | A kind of preparation method of silver nanowires |
| CN113385686B (en) * | 2021-06-08 | 2023-07-21 | 嘉兴学院 | Method for preparing silver nanowire with high length-diameter ratio by using organic amine hydrochloride as auxiliary |
| CN113732300B (en) * | 2021-08-31 | 2023-10-17 | 中硕实业(上海)有限公司 | Silver nanowire containing polyphenol compound and preparation method and application thereof |
-
2022
- 2022-05-20 CN CN202210553501.7A patent/CN114985756B/en active Active
- 2022-08-03 WO PCT/CN2022/109870 patent/WO2023221299A1/en unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106392098A (en) * | 2016-10-10 | 2017-02-15 | 苏州经贸职业技术学院 | Preparation method of nanometer silver hydrosol and treatment method for dye wastewater |
| CN114214833A (en) * | 2021-12-09 | 2022-03-22 | 西安理工大学 | Preparation method of flexible conductive fabric sensor based on silver nanowires/graphene |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2023221299A1 (en) | 2023-11-23 |
| CN114985756A (en) | 2022-09-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104495935B (en) | A kind of strip preparation method of molybdenum disulfide nano sheet layer | |
| CN109252359B (en) | Preparation method of carbon nanotube modified carbon fiber reinforced resin-based electromagnetic shielding composite material for in-situ growth of solid carbon source | |
| CN107585758A (en) | A kind of graphene aerogel and its preparation method and application | |
| CN104174864A (en) | Preparation method of nano or sub-micron silver particle powder | |
| CN110519978A (en) | A kind of Co-CNTs/ carbon fiber composite electromagnetic shield materials and preparation method thereof | |
| CN102993781A (en) | Preparation method of magnetic nano ferroferric oxide modified hollow glass microsphere | |
| CN109665525A (en) | A kind of preparation method of " dumbbell shape " iron nitrogen codope porous carbon | |
| CN105153865A (en) | Modified nanometer SiO2/epoxy-acrylate composite material preparation method | |
| CN113680326A (en) | Sulfonic acid COFs membrane and preparation method and application thereof | |
| CN114985756B (en) | Method for preparing silver nanowire based on small molecular phenolic acid at room temperature | |
| CN111842923B (en) | Preparation method of silver nanowire/biomass porous carbon electromagnetic wave absorption material | |
| CN113801631B (en) | MnCo 2 O 4 ZIF-67/Ni wave-absorbing material and preparation method thereof | |
| CN102757670B (en) | Preparation method of conductive filler | |
| CN105329950B (en) | Aluminum-doped barium strontium ferrite-poly-alpha naphthylamine composite material | |
| CN109251411A (en) | A kind of preparation method of high-strength magnetic shielding plastic | |
| CN113210623B (en) | Preparation method for synthesizing pure silver nanowire with controllable length-diameter ratio by microwave assistance | |
| CN112322339B (en) | Crude oil metal chelating agent and preparation method thereof | |
| CN114316363A (en) | Carbon nano-copper modifier and preparation method thereof | |
| CN100339305C (en) | Microwave synthesis preparation method for praseodymium hydroxide nanometer rod | |
| CN106571243B (en) | A kind of mesoporous iron oxide/manganese oxide/carbon composite nano-material, preparation method and applications | |
| CN106531460B (en) | A kind of mesoporous nickel oxide/manganese oxide/carbon nano-composite material, preparation method and applications | |
| CN106571241B (en) | A kind of mesoporous cobalt oxide/manganese oxide/carbon composite nano-material, preparation method and applications | |
| CN111302329B (en) | Composite material, preparation method and application thereof | |
| AU2021103725A4 (en) | An electromagnetic wave absorbing material based on magnetic nanoparticles/graphene/carbon fiber composites | |
| CN115206692B (en) | Preparation method and application of methoxy compound and modified carbon nano tube composite material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |